1、 KSKSKSKS SKSKSKS KSKSKS SKSKS KSKS SKS KS 2006 11 17 http:/www.kats.go.krKS I ISO 16590 KS I ISO 16590: 2006 (2011 ) I ISO 16590: 2006 : ( ) ( ) KIST ( ) : (http:/www.standard.go.kr) : :2001 12 18 :2006 11 17 :2011 12 26 2011-0623 : : ( 02- 509-7270) (http:/www.kats.go.kr). 10 5 , . ICS 13.060.50 K
2、S I ISO 16590: 2006(2011 ) Water quality Determination of mercury Methods involving enrichment by amalgamation 2000 1 ISO 16590 Water quality Determination of mercury Methods involving enrichment by amalgamation . . . . 1. . , 4 . . , 0.01 g/L 1 g/L . . 0.45 m . . , SnCl2 4 NaBH4 . / , . , (cuvette)
3、 . 253.7 nm . . 2. . . . IEC ISO . KS M 9112: 2006 ( ) KS M ISO 5667 1: 2006 1: KS M ISO 5667 2: 2006 2: 3. . . 4.6 . . . , FEP (FEP Perfluoroethenehexafluoropropene copolymer). . I ISO 16590: 2006 2 UV . . . 10 . . ( 25 ) . (cuvette) (cuvette) IR . (matrix) . 1 . 4 (II) . 1 . . 4 . . 1 (matrix) NaB
4、H4 NaBH4SnCl2 0.5 mol/L HCl 5 mol/L HCl 0.2 g/L Fe(III) 0.5 mol/L HCl (mg/L) Cu(II) 10 10 500 Ni(II) 1 500 500 Ag(I) 0.1 10 1 I 100 10 0.1 As(V) 0.5 0.5 0.5 Bi(III) 0.05 0.5 0.5 Sb(III) 0.5 0.5 0.5 Se(IV) 0.005 0.05 0.05 4. 4.1 (working range) 0.01 1 g/L . . . 4.2 (principle) , , / . , , 253.7 nm .
5、4.3 (interferences) 3. 0.1 mg/L . 4 (5. ). (II) , (digestion) . 4.4 (reagents) . . 4.4.1 4.4.2 ( ) 1.40 g/mL I ISO 16590: 2006 3 4.4.3 ( ) 1.84 g/mL 4.4.4 ( ) 1.19 g/mL 4.4.5 50 g/L 4.4.6 ( ) 5 g 500 mL (4.4.2) 1 000 mL . . 4.4.7 40 g 1 000 mL . 4.4.8 (H2NOH HCl) 10 g 100 mL . 4.4.9 5 g (SnCl2 2H2O)
6、 30 mL (4.4.4) , 100 mL . 0.5 g 100 mL . . . 30 . 4.4.10 I (Hg) 100 mg/L (HgO) 108.0 mg (4.4.6) 10 mL , 1 000 mL . 1 mL 0.1 mg . I . . 4.4.11 II (Hg) 1 mg/L I(4.4.10) 10 mL (4.4.6) 10 mL 1 000 mL . 1 mL 1 g . 1 . 4.4.12 I (Hg) 100 g/L II(4.4.11) 100 mL (4.4.6) 10 mL 1 000 mL . 1 mL 100 ng . . 4.4.13
7、 II (Hg) 10 g/L I(4.4.12) 10 mL (4.4.6) 1 mL 100 mL . 1 mL 10 ng . . 4.4.14 III (Hg) 1 g/L II(4.4.13) 10 mL (4.4.6) 1 mL 100 mL . 1 mL 1 ng . (4.4.15) . 4.4.15 (mercury calibration solutions) . 0.01 0.1 g/L . 100 mL 6 1.0 mL, 2.0 mL, 4.0 mL, 6.0 mL, 8.0 mL, 10 mL III(4.4.14) . (4.4.6) 1 mL . . 0.01
8、g/L, 0.02 g/L, 0.04 g/L, 0.06 g/L, 0.08 g/L, 0.1 g/L . . 0.1 1 g/L II(4.4.13) . 0.1 g/L, 0.2 g/L, 0.4 g/L, 0.6 g/L, 0.8 g/L, 1.0 g/L I ISO 16590: 2006 4 . . . , . 4.4.16 (reagent blank solution) (4.4.6) 10 mL 1 000 mL . digestion . . 4.4.17 (gas-washing solution) 2.5 g (II) (SnCl2 2H2O) 7.5 mL (4.4.
9、3) 50 mL . 4.4.18 (washing solution of glassware) 150 mL (4.4.2) 1 000 mL . 4.5 (4.4.18) , . 4.5.1 , . 4.5.2 . 4.5.3 . . 2 cm 15 cm( AAS .) (Quartz) . (: ) 1 2 L/min ( ). (: , ) , , , . , 100 mL, 250 mL, 1 000 mL 1 , 1 (frit, ) . , ( .) . , ( / ) . 100 mL , . 1 . (3. ). . . I ISO 16590: 2006 5 1 , 1
10、 2 L/min 2 3 (three-way stopcock) 4 : 2 cm, 15 cm 5 (gauze) 6 7 8 , 100 mL, 250 mL, 1 000 mL 9 ( ) 10 11 1 () 4.6 KS M 9112, KS M ISO 5667 1, KS M ISO 5667 2 . , , (PSF), (perfluoroethene)-6- (hexafluoropropene) (FEP) . , . (4.4.6) 10 mL 1 000 mL . pH 1 . ( ) , . 4.7 . I ISO 16590: 2006 6 . , A , B,
11、 C . . (4.6 ) 100 mL ( 1 000 mL) . 4.6 . (4.4.5) 15 mL (4.4.2) 1 mL (4.4.3) 1 mL . . 15 (4.4.7) 10 mL . 95 . . . . . . . (4.4.16) . (4.4.1) (4.4.6) . (blank problems) . ( A , B, C ). 4.8 4.8.1 (set) , (align) . 4.7 5 mL( ) (hydroxylamine chloride) (4.4.8) . 5 mL . . 30 ( ) . (aliquot) , , 200 mL . .
12、 100 mL( ) (4.4.9) 2 mL . . (1 000 mL ) 5 mL . 1 2 L/min . . . 600 . . 75 mL/min . . (4.4.15) (4.4.16) . 4.8.2 (analysis using the method of standard cali bration) . 4.4.15 . I ISO 16590: 2006 7 4.8 . . 4.8.3 , . . (spiked) , . 50 mL 0.1 g/L , 4 100 mL 50 mL (4.8.1 ). 0.5 mL, 1.0 mL, 1.5 mL (4.4.13)
13、 . 0.1 g/L, 0.2 g/L, 0.3 g/L . 4 . 4.8 (4.4.16) . 4.9 4.9.1 . pm0)(VbVAA= : (g/L) A: A0: b: Vp: (mL) Vm: (mL) 4.9.2 ( ). . . . . 4.10 0.01 g/L . 0.04 g/L, 0.20 g/L 4.11 . a) b) c) 4.10 . d) e) f) 5. 4 5.1 (working range) 0.01 1 g/L . . I ISO 16590: 2006 8 . 5.2 (principle) 4 , / , . , 253.7 nm . 5.3
14、 3. 1 mg/L , 0.1 mg/L . 1: 1 500 mL (4.4.4) 1 000 mL (III) , 500 mg/L 10 mg/L . 100 . As, Sb, Se 4 . 5.4 4.4 ( ) . 5.4.1 I 10 g 100 mL . 5.4.2 II 4.4.1 5.4.3 Mg(ClO4)2, 5.4.4 4 4 NaBH43 g , 1 g , NaOH 100 mL . 2, 3 . 4 0.02 g, 0.03 g 100 mL . 5.4.5 ( III) (III) 9 Fe(NO3)3 9H2O 14 g , 100 mL . . . 5.
15、5 (4.4.18) , . H2 . 5.5.1 (AAS) , . 5.5.2 . 5.5.3 . . 2 cm , 15 cm( AAS .) . . (: , ) . . . . 100 mL, 250 mL 2 , (wash bottle) . 100 mL ( 2 ). . ( .) . . ( / ) . I ISO 16590: 2006 9 2 . 1. (3. ). 2. . 1 2 NaBH4 3 4 5 : 2 cm, 15 cm 6 7 1 8 2 9 , 100 mL 250 mL 10 2 4 () 5.6 (4.6 ) 5.7 (4.7 ) 5.8 (procedure) 5.8.1 (set) , (align) . 4.7 5 mL( ) (hydroxylamine chloride) (4.4.8) . 5 mL . . 30 . (aliquot) , 200 mL . I ISO 16590: 2006 10 . 0.5 mL (4.4.4) 10 mL